Method of producing stannic chlorid.



1510.87 261] PATENTED JAN. 21, 1908 G. P. TOWNSEND.

METHOD OF PRODUCING STANNIG GHLORID. APFLIOATION FILED DEC. 6. 1904.

2 51mm Mann-1 PATENTED JAN. 21. 1908.

0. B; TOWNSEND. METHOD OF PRODUCING STANNIG OHLORID.

APPLICATION FILED DEC. 6. 1904 2 BHEBTS-SHEET 2.

UNITED STATES IPA-TENT. 1 OFFICE.

CLINTON PAULTOWNSEND, OF WASHINGTON, DISTRICT OF COLU BIA, ASSIGNOR, BY-MESNE ASSIGNMENTS, TO AMERICAN CAN COMPANY, A CORPORATION OF EW JERSEYm'rrion or PnonucINGs'raN m CHLORIID.

Patented Jan. 21, 1908.

To all whom it may concern? Be itknown that-I, CLINTON PAUL TOWN- SEND,a citizen of the United States, residing at Washington, in the Districtof Columbia, have invented certain-new and useful InigIOVGlXlGDtS inMethod 'of Producing-Stannic hlorid, of which the'following is aspecificatiOIl. i

This invention: is. a' method of producing and recovering stannicchlorid from' metallic tin, or from-any materialwhich contains tin inform capable of yielding achlorid of tin by reaction with chlorin. Themethod is adapted to the recovery -of stannic' chlorid from the productresulting from the detinn-ing of tin-- scra or cuttings, and will bedescribed as alpe.

plie to such product by way of examp his productas commonly obtained asa powder containing from80 to 95 per cent. of tin, largely' as metal,and relatlvely small proportions; of lead and ironor their com pounds;'Tin in this form can be refined and rendered marketable only atconsiderable cost, but is well adapted to the production of stannicchlorid according to the present method. k

For a full understanding of the invention .reference is made to theaccompanying drawin s',- wherein,,'

igure 1 is a plan view of one form of ap-- aratus for carrying out thevmethod; Fig. 2 is-a side elevationotthe same; and Figs. 3 and 4 aredetails. I

Referring to the figures, reference numerals 1-10 represent a series ofvessels or retorts of which any desired or suitable number. may beemployed: These retorts are prefer-v ably arranged in a continuousseries with a number of interposed condensers. torts shown constitute aseries and are closely grouped, suitable means being rovided for theapplication of heat as, for instance,

by embedding all rntortsin sand or other,

medium contained in a pan indicated in out line by'dotted lines 18,Figs. 1 and 2: Heat is 'ap lied tothispan in any suitable way, as by t1e contact of line gases or the application of steam under suitablepressure. retorts may, of course, be separately heated by any convenientmeans.

The retorts are indicated as consisting of acid \proof stoneware. Eachretort is pro-.

videdaivith a central aperture having a cover 19, this aperture servingfor charging. the retort an 'scharging the residuum; and two densers mayas illustrate The re- The lateral a ertures. 20, 21' for the passage ofgases an vaporized reaction products. The

vessel or retort 1 communicates directly withing retortsof a seriescommunicate only through inter osed condensers. These conbe of anydesired form, thoseillustrated comprising the pipes 22,-23 and thecollecting vessels. '1117. It will be understood that in the productionof'stannic .chloridcondensation occurs also in the exit pipe from theretort, and means for with drawing the liquid from this pipe may be usedinstead of the collecting vessels "shown; 24 is a cock shown in detailin Figs. 3, 4.

"Chlorin isintroduced through inlet 25, and is. directed into either .ofthe pipes 26 or 27 in accordance with thewqlosition of the opening 28 inthe cap 29.. enthe cock is turn'e in Fig. 3 the chlorin-introducedretort 2, and retort 9 with 10,but the remain-j at 25 will pass throughpipe 26 into thevessel 1, thence in. succession through theseveralretorts and interposed condensers, returning throu h pi e 27' tothe-cock and being directe by tlie tube 30, carried'by the cap 29, tothe outlet 31 for'waste gases. When the cock is revolved into theposition indicated in dotted lines in Fig. 3 the direction of flow throuh the retorts andcondensers is reverse the inlet and outlet remainingunchanged. Any convenientmeans for controlling and reversing the flow ofchlorin may be substituted." The pipes and collecting chambersconstitutin the condensers may, if desired be provide with a heatinsulating cover. The collecting chambers are convenientlyof glass, orother means are provided for watching the progress of the operation.

The don'denser'pi es may advantageously extend for a consl erabledistance into the retorts, as indicated lay-dotted lines in Fig. 2,whereby the current of gas is directed toward the surface of the charge.

In using the above described apparatus the operation is conductedsubstantially as fol-v lows: The retoi'ts 2 9 are charged with thetin-bearing material, preferabl as a layer of relatively slightdepth,.and ch orin is admit.- ted to the series, thechlorin beingpreferably admitted faster than it can be absorbed by the tin ina-single retort. The retorts are maintained during the distillationperiod at a suitable temperature above the vaporizing point of stannic,chlorid (114.C.), and the vaporized and entrained 'stannic chloridtofrom a gas containing chlorin.

gether with the excess of chlorin passes into the condensing andcollecting apparatus 22, 11, 23, the unconclcnsed portlons )assingthence to the retort S where a further absorption or condensationoccurs. At this stage of the operation the distillation will proceedmostrapidly in retort 2, and the number of retorts in series will be sorelated;

to the rate of supply of chlorin that the first retort will cease toyield stannic chlorid before the distillation has begun in the lastretort of the series.

For a clear understanding of the purpose of the series arrangement ofretorts and interposed condensing means it should be understood that inorder to insure a rapid production and distillation of stannic chloridit is necessary that an excess of chlorin be brought into presence ofthe tin; and that it is extremely difficult to secure a completecondensation of stannic chlorid, particularly It is, clear, therefore,'that if it be attempted to produce stannic chlorid in a single retortfollowed by a condensing system, there will result a loss of chlorinrepresenting the excess used, and a loss of stannic chlorid representingthe uncondensed portion. -According to this in- 'vention such excess ofchlorin as is desirable for rapid and economical production anddistillation ofstannic chlorid is used, and no particular necessityexists for providing the complex apparatus which would be necessary forsecuring an approximately complete condensation of the stannic chlorid.The

: gases passing from the first condenser to the second retort ordinarilycontain both chlorin and stannic ehlorid, both of which are uicklyabsorbed or condensed in presence of t e tin in the second and followingretorts. As each retort in succession ceases to absorb chlorin andstannic chlorid it will begin the delivery of stannic'chlorid to itscondenser and the succeeding retorts. Before the last retort in serieshas ceased absorbing, one or more of the retorts first in series willhave ceased distilling and should then be recharged.

In the particular form of apparatus shown it is advisable at this stageto reverse the direction of flow of chlorin through the-retorts byrotating the cap 29 of the cock 24, permitting the chlorin to enter theretorts through pipe 27 and the waste gases to esca e through pipe 26..The retorts 9, 8, 7, 6

"wi lthen yield stannic chlorid and the freshly pendent upon the totalquantity of chlorin wvliicli'has been introduced beforereversing theflow. V

The ap aratus may be so arranged as to obviate t e necessity forreversing the flow moisture it should be dried, or, preferably,

a part or all of 'the contained moisture should be converted intohydrochloric acid. This is very conveniently ell'ected as follows: Thevessels 1 and 10 are intended to contain portions of the residue whichremains in the retorts 2-9 after the completionof the distillation. Thisresidue contains a consider able proportion of ferric chlorid, which,upon contact with ,wet chlorin at a suitable temperature, reacts withthe contained moisture to produce hydrochloric acid as follows;

X01, 3H,o+ 219601, x01 mo 61-101.

This is advantageous because the reaction is accelerated. by thepresence of hydrochloric acid, and also because that portion of thechlorin which would otherwise be lost as ferric chlorid is recovered asstannic chlorid It is, of course, not essential that the vessels 110 fortreating the moist chlorin should be grouped with the distillingretorts.

Instead of stoneware. retorts, retorts of lead or of iron lined withlead, or such ves sels as are employed as generators for chlorin by themanganese dioxid method may be used.

It the chlorin bc-substantially undiluted a wide range of temperaturesabove the vaporizing point of stannic chlorid is applicable;

if, however, the chlorin be diluted with a a "tion pipe introduced intothe central aper ture of the retort. The heat developed by the reactionbetween fresh bodies of tin and chlorin is frequently sufficient to meltthe tin, whereby the retortsare endangered: these may be protected byapr-"ing to the interior surface a layer of a Suita. a material such asasbestos aper, cement, etc, indicated at 32 in Fig. 2. n case theretorts are independently heated heat will preferably be applied only ise condensed vapor into presence of tin-bearing rid, which material,substantially as described.

2. The method of producing stannic chlorid,- which consists insubjecting a tin-bear-- ing material to the. action of an excess ofchlorinand vaporizing stannic chlorid, condensing stannic chlorid fromthe vapor, and bringing the uricondense'd. vapor into" resence oftin-bearing material, substantialYy as described. 3. The method ofproducing'stannic chloconsists in subjecting a tin hearing material tothe action of chlorin and vaporizing stannic chlorid, condensing stannicchlorid from the vapor, and bringing the uncondensed vapor into presenceoftin-bearmg material at a temperature sufficient to vaporize stannicchlorid, substantially as described.

' 4:. The method of producing stannic chlorid, which consistsinsubjecting a tin-bearing material to the action of an excess ofchlorin and vaporizing stannic chlorid, condensing stannic chlorid fromthe vapor, and bringing the uncondensed vapor into presence oftin-bearing material ata temperature sufiicient to vaporize stannicchlorid, sub-v stantially as described 5; The method of producingstannic chlorid, which consists in subjecting a tin-bearing material tothe action of an excess of chlorin and-vaporizing stannic chlorid, con-(lensing stannic chlorid from the vapor, bringing the uncondensed vaporinto presence of tin-bearingmaterial at a'temperaturesuffi- ,absorb'e 6.The method ofproducing stannicchlo-- 171d, which-consists in'subjectinga tin-bearcient to vaporize stannic chlorid, and repeat-- mg the processuntil the excess of chlorin is substantially as described.

material to the action of chlorin and hydrochloric acid and vaporizingstannic chlorid, condensing stannic chlorid from the vapor, and,bringing the uncondensed vapor' into presence of tin-bearing material,substantially as described.

7. The method'oi producing stannic chlorid, which consists in passing astream con-'- taining separate bodies of a tin-bearing material, andshifting the point of sup ly of chlorin when the tin in any one of saidbodies is substantiallyexhausted, substantially as described.

8. The method of producing stannic chlorid, which consists inalternately passing a stream containing chlorin in contact with separatebodies of a tin-bearing materialand condensing stannic chlorid from saidstream, substantially as described.

9. The method of producing stannic chlo rid, which consists inalternately passing a, stream containing chlorin in contact withseparate bodies of a tin-bearing material and condensing stannicchloridfrom said stream, and shifting the point of supply of chlorinwhen the tin in any one of said bodies is substantially exhausted,substantially as described.

10. The method of producing stannic chlcrid which consists incontinuously supplying chlorin to a body of metallic tin-bearing material in the presence of anhydrous stannic chlorid.

11. The method of producing stannic chlorid, which consists in reactingon tin-bearing material with chlorin in presence of anhydrous stannicchlorid at a temperature above I the vaporizing point of anhydrousstannic chlorid, maintaining the reaction b supplying chlorin to thereacting mass, an recovering anhydrous stannic chlorid. I

12. Themethod of producing stannic chicrid which consists incontinuouslysupplying chlorin to a body-of metallic tin-bearing inaterial in thepresence of anhydrous stannic chlorid,. and controlling the temperatureof the reaction.

In testimonywhereof, I afiix my signature in presence of two Witnesses.CLINTUN, PAUL TOWNSEND. Witnesses:

EUGENE A. Brnnns, JULIA B; HILL.

so chlorin successively in contact with

